WO1996014270A1 - Aluminosilicates - Google Patents
Aluminosilicates Download PDFInfo
- Publication number
- WO1996014270A1 WO1996014270A1 PCT/EP1995/004195 EP9504195W WO9614270A1 WO 1996014270 A1 WO1996014270 A1 WO 1996014270A1 EP 9504195 W EP9504195 W EP 9504195W WO 9614270 A1 WO9614270 A1 WO 9614270A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- zeolite
- reacting zone
- sodium
- mixture
- solution
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/28—Phillipsite or harmotome type
Definitions
- the invention describes the preparation of alkali metal aluminosilicates, in particular crystalline aluminosilicates having the P-structure. These materials are of value as a component in detergent formulations in which they remove calcium and magnesium hardness ions by ion exchange. They also have other properties which provide additional benefits when used in detergent formulations. These aluminosilicates will be referred to as zeolite P in this description.
- the zeolite P class includes a series of synthetic zeolite phases which may be in cubic configuration (also termed B or P c ) or tetragonal configuration (also termed P but is not limited to these forms.
- the structure and characteristics of the zeolite P class are given in "Zeolite Molecular Sieves" of Donald W Breck (published 1974 and 1984 by Robert E Krieger of Florida USA) .
- the zeolite P class has the typical oxide formula:
- M is an n-valent cation which for this invention is an alkali metal, that is lithium, potassium, sodium, caesium or rubidium with sodium and potassium being preferred and sodium being the cation normally used in commercial processes.
- sodium may be present as the major cation with another alkali metal present in a minor proportion to provide a specific benefit.
- EP-A-384,070 is disclosed a process for manufacturing zeolite P having a silicon to aluminium molar ratio not exceeding 1.33 wherein a sodium aluminate solution, having a Na 2 0:Al 2 0 3 molar ratio from 1.4 to 2.0, is mixed with a sodium silicate solution, having a Si0 2 :Na 2 0 molar ratio from 0.8 to 3.4, at a temperature from 25°C to boiling point and with vigorous stirring to give a gel having the following composition:
- the gel is then aged for 0.5 to 10 hours at a temperature above 70°C, the crystalline sodium aluminosilicate thus formed being then washed and dried.
- EP-A-565,364 is disclosed a process for industrial production of P zeolite having the oxide formula
- y is the water content, comprising the steps of: i. a sodium aluminate solution having a temperature of at least 25°C is mixed with a sodium silicate solution at a temperature of at least 25°C in a stirred vessel in the presence of a slurry of P zeolite seed to form a gel having the composition,
- A1 2 0 3 (1-3.5) (preferably 1.80-2.2)Si0 2 : (1.2-7.5) (preferably 1.5-5)Na 2 0: (25 to 450) (preferably 40 to 150) H 2 0
- the invention relates to a process for manufacturing an alkali metal aluminosilicate of zeolite P type having the oxide formula
- reacting zone it is understood a reacting vessel or a zone of a plug flow reactor as for example marketed by Power Fluidics, AEA Technology, Risley, Warrington, U.K..
- the mixture obtained in the first reacting zone by adding together a sodium silicate solution and a sodium aluminate solution in the presence of zeolite P seeds has a Si0 2 /Al 2 0 3 mole ratio of more than 2.2 and, in the second reacting zone, a second sodium aluminate solution is added so as to give an overall Si0 2 /Al 2 0 3 mole ratio of less than 2.2 and a H 2 0/A1 2 0 3 mole ratio of less than 150 .
- dilute alkaline solution (8.1% Na 2 0) was placed in a 15 litre baffled flask. The solution was stirred (600rpm) and heated to 95°C. To the stirred solution, dilute silicate solution (14.7% Si0 2 , 9.4% Na 2 0, 1% w/w of zeolite P seeds), preheated at 90°C, and dilute aluminate solution (9.13% Al 2 0 3 , 12.5% Na 2 0) were simultaneously added at identical rate of 40g/minute. The zeolite P seeds in the dilute silicate solution were produced as disclosed in EP-A- 565,364.
- the dried samples were analyzed by XRD and all the samples were crystalline zeolite P.
- example 1 The procedure of example 1 was repeated except that 3 reactor pots were employed instead of 2. Samples were taken from the outlet pipe, filtered, washed an dried on an hourly basis. This continuous operation was maintained for 6 hours. The dried samples were also crystalline zeolite P.
- Example 3 The procedure of Example 3 was repeated with suitable increase in the A1 2 0 3 concentration in the aluminate stream so as to obtain a gel composition with Si0 2 /Al 2 0 3 ratio of 2.0 instead of 2.7.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BR9509613A BR9509613A (pt) | 1994-11-07 | 1995-10-24 | Processo para a fabricação de um aluminossilicato de metal álcalino de zeólito tipo p |
JP51500896A JP4104086B2 (ja) | 1994-11-07 | 1995-10-24 | アルミノ珪酸塩 |
EP95936550A EP0790958B1 (en) | 1994-11-07 | 1995-10-24 | Aluminosilicates |
AU38446/95A AU3844695A (en) | 1994-11-07 | 1995-10-24 | Aluminosilicates |
DE69506440T DE69506440T2 (de) | 1994-11-07 | 1995-10-24 | Alumosilikate |
US08/836,663 US5904914A (en) | 1994-11-07 | 1995-10-24 | Aluminosilicates |
GR990400433T GR3029346T3 (en) | 1994-11-07 | 1999-02-10 | Aluminosilicates |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9422401A GB9422401D0 (en) | 1994-11-07 | 1994-11-07 | Aluminosilicates |
GB9422401.1 | 1994-11-07 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1996014270A1 true WO1996014270A1 (en) | 1996-05-17 |
Family
ID=10763991
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP1995/004195 WO1996014270A1 (en) | 1994-11-07 | 1995-10-24 | Aluminosilicates |
Country Status (13)
Country | Link |
---|---|
US (1) | US5904914A (ko) |
EP (1) | EP0790958B1 (ko) |
JP (1) | JP4104086B2 (ko) |
KR (1) | KR100391869B1 (ko) |
CN (1) | CN1085619C (ko) |
AT (1) | ATE174006T1 (ko) |
AU (1) | AU3844695A (ko) |
BR (1) | BR9509613A (ko) |
DE (1) | DE69506440T2 (ko) |
ES (1) | ES2125669T3 (ko) |
GB (1) | GB9422401D0 (ko) |
GR (1) | GR3029346T3 (ko) |
WO (1) | WO1996014270A1 (ko) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004040061A1 (en) | 2002-10-30 | 2004-05-13 | Ineos Silicas Limited | Stabilised aluminosilicate slurries |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6432380B1 (en) | 2000-09-08 | 2002-08-13 | Albemarle Corporation | Synthesis of aluminosilicates via cofeeding an alkali metal aluminate and sodium silicate and cofeeding apparatus therefor |
KR100500729B1 (ko) * | 2002-05-31 | 2005-07-12 | 한국지질자원연구원 | 용융슬래그를 이용한 제올라이트 엔에이-피1 합성방법 |
JP4470039B2 (ja) * | 2004-05-12 | 2010-06-02 | 東ソー株式会社 | 新規構造ゼオライトおよびその合成方法 |
US7528201B2 (en) * | 2004-12-22 | 2009-05-05 | Exxonmobil Chemical Patents Inc. | Synthesis of silicoaluminophosphate molecular sieves |
CN1321891C (zh) * | 2005-09-22 | 2007-06-20 | 山东铝业股份有限公司 | 在含硅酸钠的铝酸钠溶液中制备p型沸石的方法 |
JP5613519B2 (ja) * | 2010-09-30 | 2014-10-22 | 水澤化学工業株式会社 | シリカアルミナ系凝集粒子 |
FR3063994B1 (fr) * | 2017-03-17 | 2022-01-21 | Arkema France | Procede de synthese a ensemencement multiple de cristaux de zeolithe a granulometrie controlee |
KR102220082B1 (ko) * | 2019-07-23 | 2021-02-25 | 노경태 | 신규 구조 및 타래형 모폴로지를 갖는 알루미노실리케이트 구조체, 이의 제조방법 및 이를 고정상으로 충진한 hplc 컬럼 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0384070A2 (en) * | 1988-11-03 | 1990-08-29 | Unilever Plc | Zeolite P, process for its preparation and its use in detergent compositions |
EP0565364A1 (en) * | 1992-04-09 | 1993-10-13 | Crosfield Limited | Aluminosilicates |
WO1995012546A1 (en) * | 1993-11-02 | 1995-05-11 | Crosfield Limited | Aluminosilicates |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3071434A (en) * | 1960-01-20 | 1963-01-01 | Socony Mobil Oil Co Inc | Process for makling crystalline zeolites |
US4385042A (en) * | 1979-08-06 | 1983-05-24 | Mobil Oil Corporation | Continuous reaction/separation method for nucleated growth reactions |
GB9216386D0 (en) * | 1992-07-31 | 1992-09-16 | Unilever Plc | Use of aluminosilicates of the zeolite p type as low temperature calcium binders |
DE4309656A1 (de) * | 1993-03-25 | 1994-09-29 | Henkel Kgaa | Verfahren zur Herstellung von feinstteiligen zeolithischen Alkalimetallaluminiumsilicaten |
EP0697010B1 (en) * | 1993-05-07 | 1998-12-02 | Crosfield Limited | Aluminosilicates |
GB9402160D0 (en) * | 1994-02-04 | 1994-03-30 | Unilever Plc | Aluminosilicates |
-
1994
- 1994-11-07 GB GB9422401A patent/GB9422401D0/en active Pending
-
1995
- 1995-10-24 WO PCT/EP1995/004195 patent/WO1996014270A1/en active IP Right Grant
- 1995-10-24 DE DE69506440T patent/DE69506440T2/de not_active Expired - Fee Related
- 1995-10-24 AT AT95936550T patent/ATE174006T1/de not_active IP Right Cessation
- 1995-10-24 JP JP51500896A patent/JP4104086B2/ja not_active Expired - Fee Related
- 1995-10-24 BR BR9509613A patent/BR9509613A/pt not_active IP Right Cessation
- 1995-10-24 KR KR1019970702996A patent/KR100391869B1/ko not_active IP Right Cessation
- 1995-10-24 ES ES95936550T patent/ES2125669T3/es not_active Expired - Lifetime
- 1995-10-24 EP EP95936550A patent/EP0790958B1/en not_active Expired - Lifetime
- 1995-10-24 CN CN95197104A patent/CN1085619C/zh not_active Expired - Fee Related
- 1995-10-24 US US08/836,663 patent/US5904914A/en not_active Expired - Lifetime
- 1995-10-24 AU AU38446/95A patent/AU3844695A/en not_active Abandoned
-
1999
- 1999-02-10 GR GR990400433T patent/GR3029346T3/el unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0384070A2 (en) * | 1988-11-03 | 1990-08-29 | Unilever Plc | Zeolite P, process for its preparation and its use in detergent compositions |
EP0565364A1 (en) * | 1992-04-09 | 1993-10-13 | Crosfield Limited | Aluminosilicates |
WO1995012546A1 (en) * | 1993-11-02 | 1995-05-11 | Crosfield Limited | Aluminosilicates |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004040061A1 (en) | 2002-10-30 | 2004-05-13 | Ineos Silicas Limited | Stabilised aluminosilicate slurries |
Also Published As
Publication number | Publication date |
---|---|
DE69506440T2 (de) | 1999-04-22 |
KR100391869B1 (ko) | 2003-09-19 |
KR970707042A (ko) | 1997-12-01 |
DE69506440D1 (de) | 1999-01-14 |
EP0790958A1 (en) | 1997-08-27 |
BR9509613A (pt) | 1997-10-21 |
GR3029346T3 (en) | 1999-05-28 |
AU3844695A (en) | 1996-05-31 |
ES2125669T3 (es) | 1999-03-01 |
ATE174006T1 (de) | 1998-12-15 |
EP0790958B1 (en) | 1998-12-02 |
US5904914A (en) | 1999-05-18 |
JP4104086B2 (ja) | 2008-06-18 |
JPH10509684A (ja) | 1998-09-22 |
GB9422401D0 (en) | 1995-01-04 |
CN1085619C (zh) | 2002-05-29 |
CN1171091A (zh) | 1998-01-21 |
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